Apparatus for making stannic chlorid.



E. A. SPERRY.

APPARATUS POR MAKING STANNIG GHLORID.v

APPLICATION FILED DEO. 7. 1905.

No. 877,243. PATENTBD JAN. 21, 19.05.

'2 SHEETS-SHEET 1.

Wi hwooeo c/ A I Gemmtg PATENTED JAN. 21, 1Q08.

I E. A.v SPBRRY. APPARATUS FOR MAKING STA/NIC GHLORID. APPLICATION FILED DBO. 7. 1905.

2 SHEETS-SHEET 2.

v IN A UNITED STATES PATENT OFFICE.

ANo. 877,243.

To all whom it may concern:

Be it known that I, ELMER A. SPERRY, a citizen of the United States, residing at Brooklyn, in the county of Kings and State of New York, have invented certain new and useful Improvements in Apparatus for Making Stannic Chlorid, of which the following is a specification. j

This'invention is an apparatus designed particularly for the production of chlorids of tin in an economical and expeditious manner and in accordance with the general method described and claimed in my copending application Serial Number 288,780, filed November 23, 1905.

For a full understanding of the invention reference is made to the accompanying drawings, illustrating a preferred construction and disposition of apparatus, wherein- Figure 1 is a perspective View of a form of apparatus constructed in accordance with my invention, parts being broken away and the scrubber being shown in vertical section; Fig. Z is a plan View, partly broken away on lines 2---2 and 2Q-2 of F ig. 3, of one of the reaction vessels; Fig. 3 is a vertical section of the'saiue on line 3--3 of Fig. 3; and Figs. 4 and 5 are detail views of forms of valves or cocks which may be employed.

Referring to the figures 1, 1, lsrepresent reaction vessels designed to receive a tin their combination. T he tin-beariing material may be in any desired form so long as the tin content is metallic and sullicient in amount to warrant treatment and recovery in the form herein contei'nplated.

2 is a chlorin main communicating with the several vessels by valved pipes 3', and 4, 4 are valved vapor outlets for the vessels, leading to a common vapor main 5. Discharge pipes 6, provided with vents 7, serve to maintain the liquid content of the vessels at constant level and permit it to overfiow to a vessel S wherein the liquid chlorids are separated by filtration or otherwise from any so id matter, products or undissolved residue,

Several reaction vessels are preferably inclosed, as shown, within a single tank or jacket 9, provided with means for circulation of water or a solution of a suitable temperature for maintenance of the proper teinperature within the reaction vessels 1, this arrangement having the advantage that a j transfer of heat is eilected between several Speccation of Letters Patent.

Application filed December 7. 1905. Serial No. 290.768.

bearing material and chlorin and to effect' ELMER A. SPERRY, OI" BROOKLYN, NEW YORK, ASSIGNOR TO CHEMICAL REDUCTION COMPANY, OF NEW YORK, N. Y., A CORPORATION OF NEW YORK.

APPARATUS FOR MAKING STANNIC CHLORID.

Patented Jan. 21, 1908.V

reaction vessels, the temperature of-whic'h is thereby equalized if they are in varying stages of the reaction.

As more particularly shown in Figs. 2, 3

each reaction vessel is preferably of elongated shape, having a converging ttom and a luted cover 11, -the latter carryinl a hopper 12 having its discharge nozzle 40 elov;T the liquid level within the vessel ywhichis also preferably provided with a luted coverv as indicated at 13; this hopper is provided with a jacket 14 whereby it ma for purposes hereinafter describe( 41 and 42 are respectively inletsand outlets for this jacket. Interiorly the vessel is provided with a central perforated or pervious containerVV 15 for tin or tin bearing material on each side of which are septa or partial partitions 16. These septa may conveniently be of wood sheathed with metal, and serve to partially subdivide the reaction vessel in such manner that the liquid contents are maintained in a more or less violentstate of agitation or motion. The construction Vis such as to secure a definite circulation of the liquid contents as hereinafter described. From the bottom of each reaction vesssel a pipe 17 leads to the vessel 8; the pi e 5 forming a vent therefor is jacketed for ieating or temperature control as shown. The mouth of the pipe 17 within the reactionvessel is closed by a plug 18, the kpurpose of which is to prevent the solid contents of the vessel from entering the pipe 17; the plug is not of necessity liquid tight, the retention of liquid being secured by a cock 19. The pipe 17 is in general used only for discharging the contents of the vessel, the overiiow normally oecurring through pipe 6 as above described. Pipes 6 and 17 are jacketed as shown, and are either directly heated to such ytemperature asv will maintain material passing through them in a liquidl state, or are so covered and protected against loss of heat Vas to accomplish this result.

Inasmuch as considerable heat is developed by the chlorination of tin in these reaction vessels, the columns of liquid between the tin and the septa 16, are of lesser speciiic gravity than the columns adjacent to the sides of the reaction vessels, and-a definite and effective circulation or agitation of the liquid is thereby secured, the liquid moving upwardly in contact with the tin in the container, thence transversely to the outer walls be heated J j of lthey vessel and downwardly to the lower end'of the container. Some of the material which escapes through the meshes of the perforated container 15 and also out at the lower 5 end is picked up by the circulating liquid and the reaction goes forward in the agitated masses as they circulate. These reactions are found to be most vigorous, however, 1n the centions remaining in the container being re- ,mdved in any suitable manner. Material ywhich is carried'in suspension in the liquid escapes through the overflow 6 to the reservoir Sand -is there separated as before deg20 scribed.

I have indicated at 20, 21 a series of vanes pro'ecting from the septa 16 into contact wit the container 15 and serving to support the latter at short intervals.- These vanes -25 preferably incline to the vertical, the inclination vbeingin opposite directions on opposite sides of the `container as clearly shown in Fig. 2; the purpose of this'inclination is to direct the-circulating liquid in a substantially heli-l cal path, in order that it may move from end to end of the vessel in addition to its movement of circulation'therein.-

22 indicates a series of baffles carried by the cover 11 and projecting beneath the sur- 3'5 face of the liquid in the vessel 1, these' baffles affording a restricted and tortuous path for thechlorin passing between the inlet 3 and the outlet 4. In this manner the chlorin is maintainedfor a longer period in contact 40 with the liquid chlorid, and is thereby more effectively absorbed.

As above stated, the reaction vessels are preferably maintained at such temperature ythat the hydrated and anhydrous stannic chlorids eXist therein as liquids capable of absorbingchlorin and conveying the same into contact with metallic tin inside and loutside the container 15. These liquid chlorids overflow into a jacketed filter 8, which. is maintained -at a suitable temperature; this filter ma be of any preferred construction, the form s own being provided with an external 'jacket' 23 andan interior filtering plate 24. Inorder to maintain the valves for hany dling the li uid chlorid in operative condition, any crysta lization therein must be guarded against; this is most conveniently effected by inclosing the valve in a jacketing sheath as shown at 2 5 in Fig. 5.V

The vapors arising from the reaction ves; .sels 1, together with those from the lter or reservoir-8, usually contain, in addition to any residual oruncondensed gases, a certain proportion of both anhydrous and hydrated stannic chlorids. These vapors are con- (sfo densed material-and crystals at all timesy Any ducted through a jacketed or heated plpe 5 to condensers 26, 26, referably arranged in pairs as shown in order. that they may be used alternately if required.y These condensers may be of any usual construction, and

are shown as provided'with cooling jackets f 27 and with a plurality of discharge openings 28, 29, the discharge openings 28 being for i the anhydrous stannic chlorid and the openings 29 for the convenient removal of any crystalline deposit of the hydrated chlorid'.

The separation of chlorid" of tin from the l gases in the condensers is ordinarily incomplete, and the residual portions are preferably removed by leading'the gases into contact with water in a scrubber or' tower 30. I have found it preferable inipractice to subject these gases to the action of water at. successively higher and lowerrtemperatures as,' for instance, by admitting lhot water through a lower inlet o r spray 31 and cold water through an upper inlet 32. By this means all traces of tin compounds are separated; obviously communicating scrubbers for hot and cold water .res ectively may be used, or any means may lie employedfor e'ecting the same result. The product front` the scrubber 30, collected as at 33, is astan-j nic chlorid solution the concentration of which will obviously depend upon the proportion'of water used to the stannic. chlorid in the vapors. A solution having a density of 50-60U B., being a marketable product, is readily prepared. An inverted perforated cone 34 is preferably provided in the upper adording a free outlet for the gases from the 'divided filling material 35 therein. haust fan 36 serves to maintain a diminished pressure in the scrubber 30 as compared with the pressure in the reaction vessels and thereby to-insure a movement of the gases through thesystem and a discharge of the.

residual gases. It is essential in the treatment' of these vapors that the condensation .v

or separation of the chlorids of tin should occur only in suchportions of the apparatus as areJespeci'ally designed for their recovery. In order toinsure this the vapor pipe 5, together with the valves therein, is heatedas before described. For the same reason the vapor pi e leading from the condenser to the scru ber, together with its valves, is heated. 'lhe inlet pipes 3 for the chlorin also the inlet chlorinvalves 3 are shown to bejacketed (see Figs. 2 and 3)"at ,3" so their temperature may be controlled. By this means the pipesare maintained free from consuitable forms of valves may be employed in the vapor lines; a Convenient form bein as indicated in Fig. 4 in which the jacket for the pipes is continued vover the cock in the form of a sheath 37, the cock being provided with an extension 38 whereby it may be manipulated The eX- from the exterior of the jacket. It is further advisable in order to prevent the caling or clogging from any cause of the material to be 'fed to the container to jacket the feeding device 01 hopper as shown at 14, whereby the material is maintained preferably at a temperature above the melting point ofthe hydrated chlorids. The heated portions extend into contact with the reacting masses at a point below thesurface ofthe liquid where the discharge nozzle of the hopper 12 is seen to be sealed by the liquid in Fig. 3, the surface of the liquid being shown by the dotted line immediately under 22, 22.

1. Apparatus for producing stannic chlorid comprising a reaction vessel, means out of contact with the contents of the vessel for controlling the temperature therein, feed and discharge orifices for the contents of the vessel, gas inlet and outlet pipescommunieating with the vessel above the normal liquid level therein, and exterior means for heating'said pipes.

2. Apparatus for producing stannic chlorid comprising a reaction vessel, means out of contact with the contents of the vessel for controlling the temperature therein, feed and discharge orifices for the contents of theves- Sel, jacketed gas inlet and outlet pipes communicating with the vessel above the normal .liquid vlevel therein, a valve in one of said jacketed pipes, and exterior means forheating said valve.

3. Apparatus for producing stannic chlorid comprising a reaction vessel, 'means out of contact with the contents of the vessel for controlling the temperature therein, means for imparting motion to the contents of the vessel, feed and `discharge orifices for the contents of the vessel, gas inlet and outlet pipes communicating with the vessel above the normal liquid level therein, and exterior means for heating said pipes.

4. Apparatus for producing stannic chlorid comprising a reaction vessel, a' lurality .of condensers, a conduit between t e vessel and condensers, valves for the condensers, and means for heating sald valves.

5. Apparatus for producing stannic chlo-l rid comprismg a reaction vessel, a scrubber, means for controlling the flow of the gases and vapors passing from the vessel to the' scrubber and a device for controlling the temperature of said controlling means. y

6. Apparatus for producing stannic chlorid comprising a reaction vessel and condenser communicating therewith, a scrubber, a conduit connecting the said members and meansfor heating the conduit.

7. Apparatus for producing stannic chlorid comprising a reactionvessel and condenser communicating therewith, a scrubber,

a conduit connecting the said members and such liquid, means for supplying chlorin to the said vessel, a device for introducing tin below theliquid level in such vessel and means for controlling the temperature of the vessel.

10. Apparatus for producing stannic chlorid comprising a reaction vessel, for containing a liquid, means for supplying chlorin to the said vessel, adevice for introducing tin below the liquid level in such vessel, .means for controlling the temperature of the vessel and means for heating the device.

11. In an apparatus for producing stannicv chlorid a reaction vessel, for containing a liquid, means for maintaining the liquid in a state of agitation, the vessel having a bottom outlet, a liquid tight valve in the outlet and a removable closure at the mouth of said outlet. A

- 12. Apparatus for producing stannic chlorid comprising a reaction vessel a device for maintaining tin in excess within the vessel, a conduit for introducing chlorin, a vapor escape pipe for the vessel and means for temperature control of the device and the pipe. 13., Apparatus for producing stannic chlo rid comprisingy a reaction vessel, means for maintaining a body of tin in the central portion of .the vessel, means for temperature c ontrol of the vessel, means for partially subdividing the vessel whereby a deiinite circulation of the contents is secured.

14.V A vessel for containing stannic chlorid, means for maintaining a body of tin submerged within a body of liquid therein, means for maintaining a supply of chlorin above the liquid level, means for causing m0- tion of the liquid and means for temperature control of the vessel.

15. A vessel for containing stannic chlorid means for maintaining la body of tin submerged within a body o f liquid therein, means for drawing chlorin in a restricted path-,above the liquid` level, means for causing n'ition of the liquid and means for temperature control of the vessel.

lio

16. Apparatus for producing stannic chlo- .l

container for tin in the central portion of the rid comprising a reaction vessel, a perforate vessel, a hopper connected therewith and y means for tem erature control of the hopper.

17. A vesse for containing liquid stannic chlorid, an inlet 4for tin communicating With i said vessel below the liquid level, means for l heating said inlet, an externally heated educ- I means out of contact with the, contents of the externally heated vent pipe for t chlorid, a reaction vesse vessel for'c'ontrolling the temperature therevalved. induction and eduction ipes for the vessel, jackets for eachof sai valves, and means for supplying a heating medium to said jackets.

' 19. A vessel for containing stannic chlorid, means out of contact with. the contents of the vvessel for controlling the tem .erature therein, a receptacle for said chlori( a heated conduit between' said vessel and rece 'tacle, an

e receptacle and an externallyT heated valve in said conduit;

20. .In apparatus for producing stannic a jacketed conduit, a scrubber 'having a vapor inlet connec'ted with the conduit, and means for subjecting the vapors to contactwith a solvent successively at higher and lower temperatures.

21. Apparatus for producin stannic chlorid comprising a reaction vesse a vapor outle't therefor, a condenser connected with said vapor outlet, means for separating stannic ch orid from the vapors traversin j said condenser, andgmeans for reducing t e gas pressure in said separating means.

- 2.2. Apparatus for producingstannc chlorid comprising a reaction vessel having an inlet, means for controlling ,said inlet, a vapor outlet for said reaction vessel, a condenser connected lwith said vapor outlet,

means for separating stannic chlorid from the vapors traversing said condenser, and' lio ture of lthe vessel, means for agitatin said body, and means for sup lying c lorin above thesurface of the' liquid' in said reaction vessel.

24. Apparatus rid comprising a reaction vessel for containing a tin-bearing material, and a body of an anhydrous liquid, means for controlling they 9temperature of the vessel, means for .agitating said' liquid and maintaining the tinbearing material in sus means for supplying ch vessel.

25.'l Apparatus for producin stannic' chloension therein, and orin to said reaction for producing stannic chlorid comprising a reaction vesse a condenser, y a conduit connecting said vessel and con'- 1 denser, and means Jfor heating said conduit. 26. A vessel for' containingstannic chlorid, means for maintaining a body of tin'sub-l v merged Within a body of I liquid th'erein,f means for maintaining a supply of chlorin,

means for causing motion o the 'liquid and means out of contact With the liquid for con`v trolling its temperature.

In testimony whereof I affix my signature.

in presence of tWo Witnesses.

p ELMER A. SPERRY.

Witnesses: L. A. WELLEs,

-'W. l?. PALMER. 

